WO2021200600A1 - 軟磁性合金粉末、磁心、磁気応用部品およびノイズ抑制シート - Google Patents

軟磁性合金粉末、磁心、磁気応用部品およびノイズ抑制シート Download PDF

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WO2021200600A1
WO2021200600A1 PCT/JP2021/012719 JP2021012719W WO2021200600A1 WO 2021200600 A1 WO2021200600 A1 WO 2021200600A1 JP 2021012719 W JP2021012719 W JP 2021012719W WO 2021200600 A1 WO2021200600 A1 WO 2021200600A1
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soft magnetic
magnetic alloy
alloy powder
axis length
alloy particles
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PCT/JP2021/012719
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French (fr)
Japanese (ja)
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ケン ラン
和宏 逸見
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株式会社村田製作所
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Priority to JP2022512088A priority Critical patent/JP7416212B2/ja
Priority to CN202180026050.5A priority patent/CN115362039B/zh
Priority to DE112021000677.0T priority patent/DE112021000677T5/de
Publication of WO2021200600A1 publication Critical patent/WO2021200600A1/ja
Priority to US17/935,779 priority patent/US20230025020A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/08—Metallic powder characterised by particles having an amorphous microstructure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15358—Making agglomerates therefrom, e.g. by pressing
    • H01F1/15366—Making agglomerates therefrom, e.g. by pressing using a binder
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F3/00—Cores, Yokes, or armatures
    • H01F3/08—Cores, Yokes, or armatures made from powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/35—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/05—Submicron size particles
    • B22F2304/054—Particle size between 1 and 100 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00—Details of transformers or inductances, in general
    • H01F27/24—Magnetic cores
    • H01F27/255—Magnetic cores made from particles

Definitions

  • the present invention relates to a soft magnetic alloy powder, a magnetic core, a magnetic application component, and a noise suppression sheet.
  • Magnetic application parts such as motors, reactors, inductors, and various coils are required to operate at large currents. Therefore, the soft magnetic material used for the iron core (magnetic core) of the magnetic application component is required to be difficult to saturate even when a high magnetic field is applied. Therefore, a soft magnetic alloy powder having a high saturation magnetic flux density such as Fe-3.5Si powder is preferred.
  • the average minor axis length / major axis length ratio of the soft magnetic alloy particles constituting the soft magnetic alloy powder is smaller than 1, the magnetic flux tends to be concentrated on both ends of the long axis with respect to the external magnetic field, and the magnetic saturation is achieved.
  • the shape of the particles constituting the soft magnetic alloy powder is required to be close to a spherical shape.
  • an iron core with a small coercive force is required.
  • the coercive force of the iron core is determined by the coercive force of the soft magnetic alloy powder.
  • the above-mentioned Fe-3.5Si has a problem that the coercive force is large.
  • a soft magnetic alloy having a small coercive force there is an amorphous soft magnetic alloy.
  • a soft magnetic alloy having a small coercive force and a high saturation magnetic flux density there is an Fe-based nanocrystal alloy or the like.
  • Patent Document 1 discloses a method of obtaining a soft magnetic alloy powder by pulverizing a continuous plate-shaped amorphous alloy called a thin band.
  • the soft magnetic alloy powder described in Patent Document 1 is a crushed powder of an amorphous alloy strip.
  • the thickness of the amorphous alloy strip is preferably 10 ⁇ m or more and 50 ⁇ m or less.
  • coarse pulverization, medium pulverization, and fine pulverization were sequentially performed using different pulverizers to pulverize the amorphous alloy strip, and then passed through a sieve having a mesh size of 106 ⁇ m (diagonal 150 ⁇ m).
  • a sieve having a mesh size of 106 ⁇ m (diagonal 150 ⁇ m).
  • the soft magnetic alloy particles contained in the soft magnetic alloy powder produced by the method described in Patent Document 1 have a thin band main surface close to a flat surface and a crushed surface exposed by crushing, and their boundaries are sharp. It shows that. Therefore, the soft magnetic alloy particles contained in the soft magnetic alloy powder produced by the method described in Patent Document 1 have a small ratio of minor axis length / major axis length and are not spherical particles. Therefore, the soft magnetic alloy powder produced by the method described in Patent Document 1 is easily magnetically saturated and has a large coercive force due to the shape magnetic anisotropy of the soft magnetic alloy particles. As a result, there is a problem that the iron loss of the magnetic core is large.
  • the present invention has been made to solve the above problems, and an object of the present invention is to provide a soft magnetic alloy powder which is hard to be magnetically saturated and has a good coercive force. Another object of the present invention is to provide a magnetic core containing the soft magnetic alloy powder, a magnetic application component having the magnetic core, and a noise suppression sheet containing the soft magnetic alloy powder.
  • the soft magnetic alloy powder of the present invention contains soft magnetic alloy particles having an amorphous phase.
  • the soft magnetic alloy particles have a chemical composition represented by Fe a Si b B c C d P e Cu f Sn g M1 h M2 i , and M1 is one or more elements of Co and Ni.
  • M2 is one or more of Ti, Zr, Hf, Nb, Ta, Mo, W, Cr, Al, Mn, Ag, V, Zn, As, Sb, Bi, Y and rare earth elements.
  • the magnetic core of the present invention contains the soft magnetic alloy powder of the present invention.
  • the magnetic application component of the present invention includes the magnetic core of the present invention.
  • the noise suppression sheet of the present invention contains the soft magnetic alloy powder of the present invention.
  • FIG. 1 is an SEM image of an example of the soft magnetic alloy powder of the present invention.
  • FIG. 2 is an enlarged SEM image of the portion surrounded by the broken line in FIG.
  • FIG. 3 is a perspective view schematically showing an example of a coil as a magnetic application component.
  • the soft magnetic alloy powder of the present invention will be described.
  • the present invention is not limited to the following configurations, and can be appropriately modified and applied without changing the gist of the present invention. It should be noted that a combination of two or more desirable configurations of each embodiment described below is also the present invention.
  • the soft magnetic alloy powder of the present invention contains soft magnetic alloy particles having an amorphous phase.
  • the soft magnetic alloy particles have a predetermined chemical composition, and the average minor axis length / major axis length ratio of the two-dimensional projected shapes of the soft magnetic alloy particles is 0.69 or more and 1 or less. do.
  • the soft magnetic alloy powder of the present invention contains soft magnetic alloy particles having a shape close to a sphere, it is difficult to be magnetically saturated and has a good coercive force.
  • a thin band having a predetermined chemical composition prepared by a single roll liquid quenching method is mechanically crushed to prepare a pulverized powder.
  • the crushed powder is put into a device that applies shear stress and compressive stress, and stress is applied to the contact points of a plurality of crushed particles to give plastic deformation, thereby causing a minor axis length /.
  • Soft magnetic alloy particles having a shape close to a sphere with a large ratio of major axis length can be produced.
  • the ratio of the average minor axis length / major axis length of the average two-dimensional projected shape of the soft magnetic alloy particles contained in the soft magnetic alloy powder can be set to 0.69 or more and 1 or less.
  • the soft magnetic alloy particles contained in the soft magnetic alloy powder of the present invention have a chemical composition represented by Fe a Si b B c C d P e Cu f Sn g M1 h M2 i.
  • a + b + c + d + e + f + g + h + i 100 (molar part) is satisfied.
  • Fe is an essential element for exhibiting ferromagnetic properties. If the amount of Fe is too large, the amorphous forming ability is lowered, and coarse crystal particles are generated after liquid quenching or heat treatment, and the coercive force is deteriorated.
  • a part of Fe may be replaced with M1 which is one or more kinds of elements of Co and Ni.
  • M1 is preferably 30 atomic% or less of the total chemical composition. Therefore, M1 satisfies 0 ⁇ h ⁇ 30.
  • a part of Fe is one or more of Ti, Zr, Hf, Nb, Ta, Mo, W, Cr, Al, Mn, Ag, V, Zn, As, Sb, Bi, Y and rare earth elements. It may be replaced with M2 which is. In that case, M2 is preferably 5 atomic% or less of the total chemical composition. Therefore, M2 satisfies 0 ⁇ i ⁇ 5.
  • Fe may be substituted with either M1 or M2, or may be substituted with both M1 and M2.
  • the sum of Fe, M1 and M2 satisfies 79 ⁇ a + h + i ⁇ 86.
  • Si also has the function of raising the second crystallization start temperature to widen the temperature range of heat treatment. However, if the amount of Si is too large, the amorphous forming ability is lowered and the coercive force is deteriorated. From the above, Si satisfies 0 ⁇ b ⁇ 5, preferably 0 ⁇ b ⁇ 3.
  • B (boron) is an essential element that enhances the bond strength between Fe atoms around the B atom, facilitates plastic deformation in the spheroidization process, and enhances the amorphous forming ability.
  • B is too large, plastic deformation becomes predominant and the ratio of minor axis length / major axis length deteriorates.
  • B has a small atomic weight, the saturation magnetic flux density is unlikely to decrease even if the amount is increased, but if it is too large, the saturation magnetic flux density decreases. From the above, B satisfies 7.2 ⁇ c ⁇ 12.2.
  • C is an essential element that enhances the bond strength between Fe atoms around the C atom, facilitates plastic deformation in the spheroidization process, and enhances the amorphous forming ability.
  • C is too large, plastic deformation becomes predominant and the ratio of minor axis length / major axis length deteriorates.
  • C has a small atomic weight, the saturation magnetic flux density is unlikely to decrease even if the amount is increased, but if it is too large, the saturation magnetic flux density decreases. Further, if C is too much, austenite is generated and the coercive force is deteriorated. From the above, C satisfies 0.1 ⁇ d ⁇ 3.
  • P phosphorus
  • P has the effect of reducing the average crystal grain size after heat treatment and reducing the coercive force. Furthermore, P also has an effect of enhancing the amorphous forming ability. If P is too large, the saturation magnetic flux density is lowered, the amorphous forming ability is lowered, and the coercive force is deteriorated. Further, since P has a negative enthalpy of mixing with Cu, it has an effect of uniformly dispersing Cu and promoting crystal nucleation during heat treatment. From the above, P satisfies 0.5 ⁇ e ⁇ 10.
  • Cu copper
  • Cu has the effect of promoting the formation of crystal nuclei in the first crystallization during the heat treatment, it has the effect of obtaining a crystal structure having a small average crystal grain size after the heat treatment and lowering the coercive force. If the amount of Cu is too large, the amorphous forming ability is lowered, and conversely, the coercive force is deteriorated. From the above, Cu satisfies 0.4 ⁇ f ⁇ 2.
  • Sn (tin) has the effect of facilitating brittle fracture due to shear stress and facilitating pulverization. If Sn is too small, elastic deformation becomes predominant, strain tends to accumulate, and the coercive force deteriorates. If the Sn is too large, the brittleness becomes too strong, making it difficult to form a sphere, and the saturation magnetic flux density decreases. From the above, Sn satisfies 0.3 ⁇ g ⁇ 6.
  • the soft magnetic alloy particles contained in the soft magnetic alloy powder of the present invention may further contain S (sulfur) of 0.5% by weight or less when the total component of the above chemical composition is 100% by weight.
  • S is an element having an effect of facilitating brittle fracture by shear stress and facilitating pulverization.
  • the amount of S is too large, the brittleness becomes too strong, making it difficult to form a sphere and deteriorating the magnetic characteristics.
  • the soft magnetic alloy particles contained in the soft magnetic alloy powder of the present invention may have only an amorphous phase. That is, the volume ratio of the amorphous phase to the soft magnetic alloy particles may be 100%.
  • the soft magnetic alloy particles contained in the soft magnetic alloy powder of the present invention may have a crystalline phase in addition to the amorphous phase.
  • the volume ratio of the amorphous phase to the soft magnetic alloy particles is preferably 10% or more.
  • the volume ratio of the amorphous phase to the soft magnetic alloy particles is preferably 50% or less, and more preferably 35% or less.
  • the volume ratio of the crystal phase to the soft magnetic alloy particles is preferably 90% or less.
  • the volume ratio of the crystal phase to the soft magnetic alloy particles is preferably 50% or more, and more preferably 65% or more.
  • the soft magnetic alloy particles are only broken and not spherical.
  • the particles produced by crushing a highly brittle thin band have a shape in which the main surface of the thin band remains and has an edge portion as described in Patent Document 1.
  • Patent Document 1 by satisfying the above chemical composition, in order to obtain spherical particles, it is possible to have both the property of being easily crushed in the crushing step and the property of being easily plastically deformed in the spheroidizing step.
  • Patent Document 1 the chemical composition for making the particle shape spherical has not been studied.
  • the soft magnetic alloy powder of the present invention is preferably produced as follows.
  • the raw materials used in the present invention are not particularly limited and may be reagents for research and development, such as pure iron and iron alloys used in electromagnetic steel plates and other cast products, and pure substances made of a single element. It may be a substance.
  • a raw material for Fe iron
  • electrolytic iron or a cast, rolled and cut product may be used as a raw material for Fe (iron), electrolytic iron or a cast, rolled and cut product.
  • the raw material of Si may be ferrosilicon, or a silicon wafer and a silicon piece of the raw material thereof.
  • the raw material of B (boron) may be metallic boron or ferroboron.
  • the raw material of C may be a simple substance such as graphite, an iron alloy such as pig iron, or SiC.
  • the raw material of P phosphorus
  • the raw material of Cu may be electrolytic copper, or may be a wire rod such as an electric wire or a cut product of the wire rod.
  • the raw material of Sn (tin) may be a simple metal Sn or an alloy.
  • the raw material may contain unavoidable impurity elements other than Fe, Si, B, C, P, Cu, Sn, M1 and M2.
  • the weight of the soft magnetic alloy is 100%, the weight of the unavoidable impurity element is preferably 2% or less, more preferably 1% or less, and particularly preferably 0.5% or less.
  • a typical unavoidable impurity element is O (oxygen).
  • the raw materials weighed to have the specified chemical composition are heated and dissolved to make the chemical concentration as uniform as possible.
  • the heating method is not particularly limited. It may be an induction heating furnace, an external heating type heating furnace, or an arc heating.
  • the atmosphere during heating is not particularly limited. It may be in the atmosphere or in an inert atmosphere such as nitrogen or argon. If the atmosphere contains oxygen, the chemical composition of the molten metal may change due to the oxidation reaction during heating. In particular, silicon and boron easily react with oxygen. It is preferable to determine the weighing value so that the chemical composition becomes a predetermined value after the dissolution is completed, in consideration of the element that reacts with oxygen and is discharged to the outside of the alloy in advance and the amount thereof.
  • the temperature of the alloy that has been melted into the molten metal is not particularly limited, but the temperature and holding time at which the chemical composition inside the molten metal becomes as uniform as possible may be selected.
  • the container that holds the raw materials is not particularly limited. Refractory materials such as alumina, mullite, and zirconia may be used.
  • the molten metal may be poured into a mold and cast to produce a mother alloy. It is also possible to omit the production of the mother alloy in order to reduce the production cost.
  • the mother alloy is crushed if necessary, and then the mother alloy is heated and melted.
  • the molten metal is cooled and solidified to form a thin band.
  • the method of cooling solidification is not particularly limited.
  • the thin band may be, for example, a continuous body having a length of 1 m or more, or may be plate-shaped or flake-shaped.
  • a single roll liquid quenching method or a double roll liquid quenching method may be used.
  • a cooling solidification method and conditions having a high cooling rate are preferable.
  • the thickness of the thin band is not particularly limited, but if it is too thick, it takes a long time to cool and solidify and further cool to a temperature below the crystallization start temperature, so that it is difficult to form an amorphous phase. It is preferable to make it as thin as possible. Further, the thickness of the thin band affects the time required for crushing in the next crushing step and the particle size after crushing. When producing a powder having a small average particle size, it is preferable to reduce the thickness of the thin band, but the time required for pulverization becomes long.
  • the thickness of the thin band is preferably 10 ⁇ m or more and 60 ⁇ m or less, more preferably 14 ⁇ m or more and 40 ⁇ m or less, and particularly preferably 18 ⁇ m or more and 30 ⁇ m or less.
  • the material of the cooling roll is not particularly limited. Pure copper may be selected, or a copper alloy such as beryllium copper or chromium zirconia copper may be selected.
  • a liquid such as water or oil may be circulated inside the cooling roll for cooling. The lower the temperature of the liquid such as water or oil immediately before the flow path inside the cooling roll, the faster the cooling rate can be, which is preferable. However, if the surface of the roll is defective due to dew condensation, the temperature may be higher than room temperature. Quartz, boron nitride, or the like can be selected as the material of the nozzle that supplies the molten metal to the surface of the cooling roll.
  • the nozzle shape may be a rectangular slit or a round hole.
  • the thin band preferably contains an amorphous phase, and may contain crystal grains having a body-centered cubic structure, for example.
  • the surface of the strip may have an oxide phase and may contain one or more of magnetite, wustite, silicon oxide and boron oxide.
  • the pulverization method is not particularly limited, such as a pin mill, a hammer mill, a feather mill, a sample mill, a ball mill, and a stamp mill, but the average particle size of the pulverized powder is preferably 300 ⁇ m or less.
  • the machine is not particularly limited, but a surface modification / compositing device such as a hybridization system (manufactured by Nara Machinery Co., Ltd.) is preferable.
  • the ground powder is chipped. Then, under the condition that a plurality of particles are aggregated into a single particle by plastic deformation, soft magnetic alloy particles closer to a sphere can be obtained, which is preferable.
  • a classification step may be appropriately provided before and after the crushing step and the spheroidizing treatment.
  • the classification device and the classification conditions are not particularly limited, and a sieve classification may be used or an air flow type classifier may be used.
  • the soft magnetic properties may be improved by heat-treating the soft magnetic alloy particles produced by the above method.
  • Strain is introduced inside the soft magnetic alloy particles by the crushing step and the spheroidizing step.
  • the strain introduced into the soft magnetic alloy particles increases the coercive force to increase the magnetic anisotropy.
  • the soft magnetic alloy particles are heated to a temperature at which the diffusion of atoms is promoted to maintain the temperature, so that the atoms are diffused so as to alleviate the strain and the strain can be reduced. can.
  • the first crystallization start temperature is a temperature at which a crystal phase having a body-centered cubic structure begins to be formed when the amorphous phase having the chemical composition of the present invention is heated from room temperature.
  • the first crystallization start temperature depends on the heating temperature rise rate. The faster the heating temperature rise rate, the higher the first crystallization start temperature, and the slower the heating temperature rise rate, the lower the first crystallization start temperature.
  • the saturation magnetic flux density is improved and the coercive force is lowered. Since the crystal phase is a phase in which a solute such as Si is solid-solved in ⁇ -Fe, the saturation magnetic flux density is high.
  • the volume ratio of the crystal phase to the soft magnetic alloy particles is preferably 50% or more, and particularly preferably 65% or more.
  • the volume ratio of the crystal phase to the soft magnetic alloy particles is preferably 90% or less.
  • the rest is an amorphous phase. Therefore, the volume ratio of the amorphous phase to the soft magnetic alloy particles is preferably 50% or less, and more preferably 35% or less.
  • the volume ratio of the amorphous phase to the soft magnetic alloy particles is preferably 10% or more.
  • the crystal grain size of the crystal phase is preferably 30 nm or less, more preferably 25 nm or less, and particularly preferably 20 nm or less. On the other hand, the crystal grain size of the crystal phase is, for example, 5 nm or more.
  • the rate of temperature rise is preferably, for example, 20 ° C./min or more and 100,000 ° C./min or less, and more preferably 100 ° C./min or more and 50,000 ° C./min or less.
  • the second crystallization reaction is started.
  • an Fe-B compound or an Fe-P compound is produced. Since the Fe-B compound and the Fe-P compound have hard magnetism, the coercive force of the powder increases. Therefore, it is preferable to carry out the heat treatment at a temperature equal to or higher than the first crystallization start temperature and lower than the second crystallization start temperature.
  • the atmosphere of the heat treatment is not particularly limited, but it is preferable that the oxygen concentration is low.
  • the atmosphere contains oxygen, an oxide layer is formed on the surface of the soft magnetic alloy particles. While the oxide layer functions as an insulating film, it lowers the saturation magnetic flux density.
  • the cooling conditions for heat treatment are not particularly limited.
  • the heating principle of the heat treatment furnace is not particularly limited, but it is preferable to satisfy the above-mentioned heating rate.
  • the infrared lamp annealing furnace can raise the temperature at a maximum of 1000 ° C./min.
  • the soft sample may be brought close to or in contact with a preheated solid substance.
  • the heated gas may be brought into contact with the sample. It may be microwave heating or induction heating by electromagnetic waves having a wavelength shorter than that of microwaves.
  • the ratio of the minor axis length / major axis length of the soft magnetic alloy particles is measured from the two-dimensional projection drawing of the appearance of the soft magnetic alloy particles.
  • a method of analyzing an image taken with a scanning electron microscope (SEM) a method of analyzing an image taken with a microscope, and a particle image analysis system such as Shimadzu's iSpec DIA-10, FPIA, and VHX-6000. There is a method using.
  • the contours of the particles are extracted from the image taken by the SEM, and the ratio of the minor axis length / the major axis length is analyzed by the automatic image analysis software "WinROOF".
  • the ratio of length / major axis length can be obtained in the same manner as the soft magnetic alloy particles by polishing the cross section of the magnetic core and imaging with an SEM or the like.
  • FIG. 1 is an SEM image of an example of the soft magnetic alloy powder of the present invention.
  • FIG. 2 is an enlarged SEM image of the portion surrounded by the broken line in FIG.
  • the ratio (Y / X) of the minor axis length Y to the major axis length X is determined as shown in FIG.
  • the long axis of the soft magnetic alloy particles 10 means the longest straight line among the straight lines connecting arbitrary two points on the contour of the particles.
  • the minor axis of the soft magnetic alloy particle 10 means a straight line that passes through a point that divides the major axis into two equal parts and is orthogonal to the major axis among the straight lines connecting arbitrary two points on the contour of the particles. ..
  • the average major axis length and the average minor axis of the soft magnetic alloy particles are as long as the ratio of the average minor axis length / major axis length of the soft magnetic alloy particles satisfies 0.69 or more and 1 or less.
  • the length is not particularly limited.
  • the average major axis length of the soft magnetic alloy particles is, for example, in the range of 25 ⁇ m or more and 45 ⁇ m or less, and the average minor axis length of the soft magnetic alloy particles is, for example, in the range of 25 ⁇ m or more and 45 ⁇ m or less.
  • the use of the soft magnetic alloy powder of the present invention is not particularly limited.
  • the soft magnetic alloy powder of the present invention can be processed into, for example, a magnetic core used for magnetic application parts such as a motor, a reactor, an inductor, and various coils, and a noise suppression sheet.
  • a magnetic core containing the soft magnetic alloy powder of the present invention, a magnetic application component provided with the magnetic core, and a noise suppression sheet containing the soft magnetic alloy powder of the present invention are also included in the present invention.
  • a magnetic core can be formed by kneading a binder dissolved in a solvent and a soft magnetic alloy powder, filling the mold, and applying pressure.
  • the resin constituting the binder is not particularly limited, and may be a thermosetting resin such as an epoxy resin, a phenol resin, or a silicon resin, or a thermoplastic resin and a thermosetting resin may be mixed.
  • the molded magnetic core can be heated after drying the excess solvent to increase the mechanical strength. Heat treatment may be performed in order to alleviate the strain of the soft magnetic alloy particles introduced by the pressure during molding. For example, heat treatment at a temperature of 300 ° C. or higher and 450 ° C. or lower under the condition that the resin does not burn or volatilize and adversely affect the magnetic characteristics can easily alleviate the strain.
  • FIG. 3 is a perspective view schematically showing an example of a coil as a magnetic application component.
  • the coil 100 shown in FIG. 3 includes a magnetic core 110 containing the soft magnetic alloy powder of the present invention, and a primary winding 120 and a secondary winding 130 wound around the magnetic core 110.
  • the primary winding 120 and the secondary winding 130 are bifilar-wound around the magnetic core 110 having an annular toroidal shape.
  • the structure of the coil is not limited to the structure of the coil 100 shown in FIG.
  • one winding may be wound around a magnetic core having an annular toroidal shape.
  • the structure may include a body containing the soft magnetic alloy powder of the present invention and a coil conductor embedded in the body.
  • Example 1 The raw materials were weighed to a predetermined chemical composition. The total weight of the raw materials was 150 g. Myron (purity 99.95%) manufactured by Toho Zinc Co., Ltd. was used as the raw material for Fe. As the raw material of Si, granular silicon (purity 99.999%) manufactured by High Purity Chemical Laboratory Co., Ltd. was used. As the raw material of B, granular boron (purity 99.5%) manufactured by High Purity Chemical Laboratory Co., Ltd. was used. As the raw material of C, powdered graphite (purity 99.95%) manufactured by High Purity Chemical Laboratory Co., Ltd. was used.
  • As the raw material of P massive iron phosphide Fe 3 P (purity 99%) manufactured by High Purity Chemical Laboratory Co., Ltd. was used.
  • As the raw material for Cu chip-shaped copper (purity 99.9%) manufactured by High Purity Chemical Laboratory Co., Ltd. was used.
  • As the raw material of Sn granular tin (purity 99.9%) manufactured by High Purity Chemical Laboratory Co., Ltd. was used.
  • the above raw material was filled in an alumina crucible (U1 material) manufactured by TEP, heated by induction heating until the sample temperature reached 1300 ° C., and held for 1 minute to dissolve.
  • the dissolution atmosphere was argon.
  • the molten metal obtained by melting the raw materials was poured into a copper mold and cooled and solidified to obtain a mother alloy.
  • the mother alloy was crushed with a jaw crusher to a size of about 3 mm to 10 mm. Subsequently, the mother alloy crushed by the single roll liquid quenching device was processed into a thin band. Specifically, 15 g of a mother alloy was filled in a nozzle made of a quartz material, and the mixture was heated to 1200 ° C. by induction heating in an argon atmosphere to dissolve it.
  • the molten metal obtained by melting the mother alloy was supplied to the surface of a cooling roll made of a copper material to obtain a thin band having a thickness of 15 ⁇ m to 25 ⁇ m and a width of 1 mm to 4 mm.
  • the hot water gas pressure was 0.015 MPa.
  • the hole diameter of the quartz nozzle was 0.7 mm.
  • the peripheral speed of the cooling roll was set to 50 m / s.
  • the distance between the cooling roll and the quartz nozzle was 0.27 mm.
  • the length of the strips varies depending on the chemical composition, and some samples have a plurality of short strips of about 50 mm and some samples have a length of 5 m or more.
  • the obtained thin band was crushed using a sample mill SAM manufactured by Nara Machinery Co., Ltd.
  • the rotation speed of the SAM was 15,000 rpm.
  • the pulverized powder obtained by pulverization by SAM was sphericalized using a surface modification / compositing device.
  • a hybridization system NHS-0 manufactured by Nara Machinery Co., Ltd. was used as the surface modification / composite device.
  • the rotation speed was 13000 rpm, and the processing time was 30 minutes.
  • the crushed powder was passed through a sieve having a mesh size of 38 ⁇ m to remove coarse particles remaining on the sieve.
  • the powder was passed through a sieve having a mesh size of 20 ⁇ m to remove fine particles that had passed through the sieve, and the soft magnetic alloy powder remaining on the sieve was recovered.
  • the obtained soft magnetic alloy powder was used as samples 1 to 55.
  • the appearance of the soft magnetic alloy particles contained in the soft magnetic alloy powder was imaged using a scanning electron microscope manufactured by JEOL Ltd.
  • the contours of the obtained SEM image were extracted using the image processing software "WinROOF", and 100 soft magnetic alloy particles were selected except for the particles whose contours were inaccurate due to the overlap of the soft magnetic alloy particles.
  • the average minor / major length ratio was calculated by automatic analysis.
  • VSM vibration sample type magnetization measuring instrument
  • the apparent density ⁇ was measured by the pycnometer method.
  • the replacement gas was He.
  • the saturation magnetic flux density Bs was calculated from the values of the saturation magnetization Ms measured by VSM and the apparent density ⁇ measured by the pycnometer method using the following equation (1).
  • Bs 4 ⁇ ⁇ Ms ⁇ ⁇ ⁇ ⁇ ⁇ (1)
  • the coercive force Hc was measured with a coercive force magnet K-HC1000 manufactured by Tohoku Steel Co., Ltd.
  • the capsule for powder measurement was filled with soft magnetic alloy powder and compacted so that the powder did not move when a magnetic field was applied.
  • the volume ratio Va of the amorphous phase was determined by the following equation (2), where Ia was the area strength of the halo due to the amorphous phase and Ic was the (110) peak area strength of the crystal phase having a body-centered cubic structure.
  • Table 1 shows the chemical composition of samples 1 to 10, the average minor axis length / major axis length ratio, the volume ratio Va of the amorphous phase, the saturation magnetic flux density Bs, and the coercive force Hc.
  • Table 1 the sample numbers marked with * are comparative examples outside the scope of the present invention. The same applies to Table 2-1 and Table 2-2 and Table 3.
  • Example 2 The first crystallization start temperature and the second crystallization start temperature of Samples 1 to 55 were measured by a differential scanning calorimeter (DSC). The temperature was raised from room temperature to 650 ° C. at 20 ° C./min, and the heat generation of the sample at each temperature was measured. At this time, a platinum sample container was used. Argon (99.999%) was selected as the atmosphere, and the gas flow rate was 1 L / min. The amount of the sample was 15 mg to 20 mg. The intersection of the tangent of the DSC curve below the temperature at which the heat generation due to crystallization starts and the maximum slope tangent at the rise of the heat generation peak of the sample due to the crystallization reaction was defined as the crystallization start temperature.
  • DSC differential scanning calorimeter
  • the sample was heat-treated at a temperature 20 ° C. higher than the measured first crystallization start temperature to generate nanocrystals from the amorphous phase. As a result, the amorphous phase and nanocrystals coexisted in the sample.
  • As the heat treatment furnace an infrared lamp annealing furnace RTA manufactured by Advance Riko Co., Ltd. was used. The heat treatment atmosphere was argon, and carbon was used as the infrared susceptor. 2 g of the sample was placed on a carbon susceptor having a diameter of 4 inches, and a carbon susceptor having a diameter of 4 inches was further placed on the sample. The control thermocouple was inserted into the thermocouple insertion hole in the lower carbon susceptor. The heating rate was 400 ° C./min. The holding time at the heat treatment temperature was 1 minute. The cooling was natural cooling, and the temperature reached 100 ° C. or lower in about 30 minutes.
  • the chemical composition, average minor axis length / major axis length ratio, saturation magnetic flux density Bs and coercive force Hc of each sample were measured by the same method as in Example 1.
  • the crystal state of the soft magnetic alloy powder after the heat treatment was confirmed using an X-ray diffractometer.
  • the average statistical particle size of the ⁇ —Fe crystal phase was calculated from the diffraction peak using the Scherrer equation shown in (4) below.
  • the holding power can be lowered.
  • the amount of C is too large as in the sample 25, the plastic deformation becomes predominant and the ratio of the minor axis length / the major axis length deteriorates.
  • sample 18 has a high holding power because c + d is small.
  • the samples 21 and 26 have a large c + d, the plastic deformation becomes predominant and the ratio of the minor axis length / the major axis length deteriorates.
  • the coercive force can be lowered.
  • the amount of P is too large as in the sample 30, the saturation magnetic flux density decreases.
  • the holding power of samples 31 to 34 can be lowered by containing Cu.
  • the amount of Cu is too large as in the sample 34, the amorphous forming ability is lowered, and conversely, the coercive force is deteriorated.
  • the holding power can be lowered.
  • the Sn is too large as in the sample 35, the ratio of the minor axis length / the major axis length deteriorates, and the saturation magnetic flux density also decreases.
  • a part of Fe is a part of Ti, Zr, Hf, Nb, Ta, Mo, W, Cr, Al, Mn, Ag, V, Zn, As, Sb, Bi, Y and rare earth elements.
  • M2 which is one or more kinds of elements, a soft magnetic alloy powder having good saturation magnetic flux density and holding power can be formed.
  • the amount of replacement with M2 is large as in the samples 41, 43, 45, 47, 49, 51, 53 and 55, the saturation magnetic flux density is lowered and the holding power is increased.
  • Example 3 An insulating film was formed on the surface of the soft magnetic alloy powder produced in Example 2. To 30 g of the soft magnetic alloy particles, 8.5 g of isopropyl alcohol (IPA), 8.5 g of 9% aqueous ammonia, and 1.14 g of 30% plysurf AL were mixed. Then, a mixed solution of 7.9 g of IPA and 2.1 g of tetraethoxysilane (TEOS) was mixed in 3 portions of 1.0 g each, and filtered through a filter paper. The sample recovered with the filter paper was washed with acetone, dried by heating at a temperature of 80 ° C. for 60 minutes, and heat-treated at a temperature of 140 ° C. for 30 minutes to obtain a composite soft magnetic alloy powder.
  • IPA isopropyl alcohol
  • TEOS tetraethoxysilane
  • the above composite soft magnetic alloy powder was processed into a toroidal-shaped magnetic core.
  • the weight of the composite soft magnetic alloy powder was 100% by weight, 1.5% by weight of the phenol resin PC-1 and 3.0% by weight of acetone were mixed in a mortar.
  • the sample is filled in a mold and hot-molded at a pressure of 60 MPa and a temperature of 180 ° C to have an outer diameter of 8 mm and an inner diameter of 4 mm. It was molded into a toroidal shape.
  • the relative initial magnetic permeability of the magnetic core was measured with an impedance analyzer E4991A manufactured by Keysight Co., Ltd. and a magnetic material test fixture 16454A.
  • a copper wire was wound around the magnetic core to measure core loss (iron loss).
  • the diameter of the copper wire was 0.26 mm.
  • the number of turns of the primary winding for excitation and the number of turns of the secondary winding for detection were the same in 20 turns, and bifilar winding was applied.
  • the frequency condition was 1 MHz, and the maximum magnetic flux density was 20 mT.
  • Table 3 shows the coercive force and core loss of the magnetic core.
  • sample 1 the coercive force of the magnetic core is high and the core loss is high.
  • sample 5 the coercive force of the magnetic core is low and the core loss is low.
  • the sample 56 is a comparative example obtained by pulverizing with a sample mill. In sample 56, the ratio of minor axis length / major axis length was small, the filling rate was poor, and the core loss was high, making measurement impossible.
  • Soft magnetic alloy powder 10 Soft magnetic alloy particles 100 Coil 110 Magnetic core 120 Primary winding 130 Secondary winding X Long axis length Y Short axis length

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